CN104445320A - Composite salt treatment and comprehensive utilization process of insoluble potassium-enriched minerals - Google Patents

Composite salt treatment and comprehensive utilization process of insoluble potassium-enriched minerals Download PDF

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CN104445320A
CN104445320A CN201410743448.2A CN201410743448A CN104445320A CN 104445320 A CN104445320 A CN 104445320A CN 201410743448 A CN201410743448 A CN 201410743448A CN 104445320 A CN104445320 A CN 104445320A
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potassium
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CN104445320B (en
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刘耀驰
莫红兵
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Central South University
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Abstract

The invention discloses a composite salt treatment and comprehensive utilization process of insoluble potassium-enriched minerals. The process comprises the following steps: mixing insoluble potassium-enriched minerals with composite salt containing calcium salt and sodium salt, and then roasting at high temperature; performing water leaching on a roasted product, and then performing solid-liquid separation I to obtain a solid I and a liquid I, wherein the solid I is used for preparing aerated bricks or Portland cement additives, the liquid I is used for separating out precipitates by adjusting a pH value and is subjected to solid-liquid separation II to obtain a solid II and a liquid II, and the solid II is further prepared into Al2(SO4)3 or Al2O3; and preparing K2SO4 or K2CO3 by performing condensation crystallization or salt precipitation on the liquid II. According to the process disclosed by the invention, the insoluble potassium-enriched minerals are subjected to roasting treatment by the composite salt containing the calcium salt and sodium salt, and water leaching is combined to ensure that potassium, aluminum and silicon in the insoluble potassium-enriched minerals are fully separated, and meanwhile, aluminum products and potassium products with relatively high purity can be obtained; and by adopting the process, the comprehensive recovery and utilization of insoluble potassium-enriched mineral resources can be achieved.

Description

A kind of composite salt process of insoluble kalium contained mineral and comprehensive utilization process
Technical field
The present invention relates to a kind of composite salt process and comprehensive utilization process of insoluble kalium contained mineral, belong to insoluble kalium contained mineral technical field of resource comprehensive utilization.
Background technology
The potassium-bearing mineral of insoluble potassium rich rock is mainly microline, and its crystal-chemical formula is K [AlSi 3o 8], theoretical composition (massfraction): SiO 264.7%, Al 2o 318.4%, K 2o 16.9%, triclinic(crystalline)system, [Si (Al) O in crystalline structure 4] tetrahedron connects to tetra-atomic ring.Therefore, the target of potassium rich rock comprehensive utilization destroys potassium felspar sand structure with minimum energy, and realize SiO as far as possible 2, Al 2o 3, K 2the recycling of O tri-kinds of components, what wherein utility value was the highest is potassium.
Although potassium is extensive by approach, world's sylvite output more than 90% is used as potash fertilizer, and as everyone knows, potassium is one of three large nutritive elements.The extraction of potassium is in the world mainly derived from soluble potassium salt deposit, but worldwide soluble potassium distributed pole is uneven, mainly in Canada, France, Germany, member country of the Commonwealth of Independent States, the U.S. etc., accounts for more than 96% of world saving.To 2012, whole world water-soluble potassium salt reserve amounted to K 2o is 95.52 hundred million t; Chinese Potassium Industry reserves are 2.1 hundred million t, find out resource reserve 6.54 hundred million t, are mainly distributed in the Cha Er Han Salt Lake of Chaidamu Basin, Qinghai Province and the salt lake, Lop Nur of Tarim Basin In Xinjiang.
Sylvite is one of China's two kinds of nonmetallic minerals the most in short supply.2003, domestic production potash fertilizer 164.5 ten thousand t, import potash fertilizer 623.5 ten thousand t, accounted for 79.1% of apparent consumption.Within 2007, potash fertilizer import volume accounts for 71.8% of Apparent con-sumption.China's soluble potassium salt reserve is low, Jin Zhan world total reserves about 2.2%, although China increases the exploitation dynamics of potassium in recent years, as Salt Lake Potash Repone K, CITIC Guoan's potash magnesium sulphate fertilizer, Lop Nur sylvite company, Shanshan, Xinjiang county (the universal group in Zhejiang) etc., but current external dependence degree is still more than 50%.On the other hand, China's insoluble potassic mineral aboundresources, of a great variety, known potassium-bearing mineral comprises potassium felspar sand, white garnet, biotite, alunite, glaukonine, illite etc.; Main potassium bearing rock has potassium-bearing shale, hydromica tonstein, all kinds of potassic volcanic rock and irruptive rock etc.These insoluble potassic mineral resources almost spread all over the country each provinces, municipalities and autonomous regions, and according to statistics, upper table reserves reach tens billion of ton.Therefore, utilizing insoluble kalium contained mineral to produce sylvite, is the strategic demand ensureing Agricultural Sustainable Development in China.
The research utilizing insoluble kalium contained mineral to produce sylvite technology exceedes a century, although hydrofluoric acid and sodium hydroxide are all effective auxiliary agents of decomposing of potassium feldspar, because its corrodibility is extremely strong, cost of material is high without economic worth.Still there is material impact so far or mainly contain potassium felspar sand-nepheline-CaCO in lasting research 3high-temperature sintering process, potassium felspar sand-CaSO 4-CaCO 3high-temperature sintering process, potassium felspar sand-Na 2cO 3/ K 2cO 3high-temperature sintering process, potassium felspar sand-H 2sO 4-CaF 2low temperature acid hydrolyzation, potassium felspar sand-Ca (OH) 2-H 2o static hydrothermal method etc.
Insoluble kalium contained mineral is produced sylvite and is had a extensive future, in China, the patent only utilizing potassium felspar sand to prepare sylvite at present just reaches nearly 60, as Chinese Academy Of Sciences Process Engineering Research Institute, the Dan Jun such as Kunming Inst. of Metallurgy and Luoyang Fu Jia Science and Technology Ltd. have series of patents, as " a kind of method CN201010590230.X fully utilizing potassium felspar sand production potash fertilizer and aluminum oxide ", " potassium felspar sand comprehensive utilization novel process CN201110430995.1 ", " utilize the technique CN201310527135.9 of potassium felspar sand preparing potassium sulfate ", in research, horse great writing team has done long-term continuing to the utilization of domestic representative potassium rich rock resource and has studied in nearly 20 years, successively having carried out pure alkali sintering process prepares K 2cO 3by-product 13X molecular sieve, pure alkali sintering process produce K 2cO 3byproduct mineral matter polymeric material, hydro-thermal Ca (OH) 2method produces K 2cO 3(or mineral base saltpetre) by-product tobermorite powder, hydro-thermal NaOH method produce K 2cO 3and Na 2cO 3and by-product metallurgical-grade aluminum oxide, hydro-thermal KOH method produce K 2sO 4by-product calcined kaolin etc. [horse great writing etc. potassium rich rock is produced sylvite and is studied 20 years: reviews and prospects. ground leading edge, 2014,21 (5): 236-254].
Although existing a large amount of technological development and patent, above-mentioned technological process is mostly difficult to realize large-scale industrialized production, comprehensively analyzes, and main exist following deficiency: (1) energy consumption and material consumption are comparatively large, as high-temperature sintering process, adopts Na 2cO 3/ K 2cO 3also there is the problems such as raw materials cost is high, magazins' layout is complicated in the high temperature sintering carried out; (2) acidic process causes cost high because foreign matter content is high, and equipment corrosion is serious, Environmental compatibility is poor, the especially acidic process of fluoride, and this problem is especially serious; (3) tailings emission problem is difficult point in acidic process, for alkaline process, because calcium silicate slag can by-product silicate cement and reducing costs; (4) the main deficiency of the hydrothermal method that current research is more is that potassium feldspar decomposition is incomplete, product K 2o nutrient content low and in strong basicity (pH>=10), reaction time long-acting rate low, be difficult to realize large-scale industrial and produce.
Summary of the invention
For in prior art to the defect that the treatment process of insoluble kalium contained mineral exists, the object of the invention is to be that providing a kind of carries out calcination process and Bound moisture leaching by the composite salt containing calcium salt and sodium salt to insoluble kalium contained mineral, potassium in insoluble kalium contained mineral, aluminium, silicon are fully separated obtain aluminium product and the potassium product of higher degree simultaneously, the technique of insoluble kalium contained mineral resource comprehensive utilization and utilization can be realized.
The invention provides a kind of composite salt process and comprehensive utilization process of insoluble kalium contained mineral, this technique, after being mixed with the composite salt containing calcium salt and sodium salt by insoluble kalium contained mineral, is carry out roasting under the condition of 850 ~ 1650 DEG C in temperature; Product of roasting, after water logging goes out, carries out solid-liquid separation I, obtains solid I and liquid I; Solid I is for the preparation of aerated bricks or silicate cement addition material, and liquid I is after regulating pH to 5.5 ~ 9.5, and carry out solid-liquid separation II, obtain solid II and liquid II, solid II is prepared into Al further 2(SO 4) 3or Al 2o 3; Liquid II is by condensing crystal or the preparation K that saltouts 2sO 4or K 2cO 3; Described calcium salt is one or more in any calcium salt outside the villaumite of deliming and villiaumite, and described sodium salt is one or more in any sodium salt except the villaumite of sodium, villiaumite and carbonate.
Composite salt process and the comprehensive utilization process of insoluble kalium contained mineral of the present invention also comprise following preferred version:
Mass ratio 0.3 ~ the 1.0:1 of insoluble kalium contained mineral and the composite salt containing calcium salt and sodium salt in preferred scheme.
The mass ratio containing calcium salt and sodium salt in the composite salt of calcium salt and sodium salt in preferred scheme is 100:2 ~ 25.
In preferred scheme, roasting time is less than 3h.
In preferred scheme in liquid II sodium mass percent concentration higher than potassium mass percent concentration 5% time, in liquid II, add Repone K carry out replacement(metathesis)reaction to reduce follow-up K 2sO 4or K 2cO 3sodium content in product.
In preferred scheme, the leaching of product of roasting to be mixed with the liquid-solid mass ratio 4 ~ 12:1 of insoluble kalium contained mineral raw ore by water by product of roasting to leach.
In preferred scheme, solid I mainly comprises calcium and silicon composition, according to prepare aerated bricks or silicate cement addition material need simply washed by existing technique, after the process such as ball milling, may be used for preparing aerated bricks or silicate cement addition material.
Mainly comprise sodium, potassium and aluminium in liquid I in preferred scheme, the foreign matter content such as silicon, phosphorus of sepn process complexity is extremely low.
In preferred scheme, solid II is for being rich in aluminium slag, and aluminium hydroxide content is minimum reaches 80%, is usually all greater than 95%, is processed further obtain Al by existing maturation process 2(SO 4) 3or Al 2o 3.
In preferred scheme, solid-liquid separation I and solid-liquid separation II can be selected from filtration, press filtration, dense or sedimentation, the separation method such as centrifugal independently of one another.
Hinge structure, major technique advantage of the present invention: technique of the present invention adopts the suitable composite salt be made up of calcium salt and sodium salt insoluble kalium contained mineral to be carried out to the roasting of proper temperature first, again in conjunction with water logging, potassium can be realized, aluminium is effectively separated with the difficult separating impurity such as silicon, obtain aluminium product and the potassium product of higher degree simultaneously.The roasting in the conditions of the invention of insoluble kalium contained mineral, only just need can obtain by water logging the aqueous solution containing K and Al, foreign matter content extremely low (see embodiment table 2) in the aqueous solution, its general foreign matter content is lower than 20mg/L, even the impurity Si of the most difficult separation, its content is not also higher than 30mg/L, therefore rear end Al with K be separated easy, Al and the K product purity of producing is high, and greatly reduce production cost on the whole, industrialization prospect is wide.Meanwhile, not fluoride in technological process, produces the waste residue that produces and can be used for preparing aerated bricks or as silicate cement addition material, the Environmental compatibility of whole technique is good, achieves the comprehensive utilization of insoluble kalium contained mineral through suitable pre-treatment.
Accompanying drawing explanation
The composite salt process that [Fig. 1] is insoluble kalium contained mineral and the process flow sheet of comprehensive utilization.
Embodiment
Following specific embodiment is intended to further illustrate content of the present invention, instead of the scope of restriction the claims in the present invention protection.
Embodiment 1
By the calcium salt that 1000g calcium sulfate and 400g calcium carbonate mix, composite salt is formed with 100 SODIUMNITRATE, mix with 1000g potassium felspar sand breeze, control maturing temperature 1100 DEG C, roasting 1.5h, roasting material carries out 4h water logging, and the mass ratio controlling water and raw ore is 6:1, processes out rear acquisition solid I and 5600mL liquid I after filtration.In liquid I, Al content is 7367mg/L, K content be 11620mg/L, Na content is 3600mg/L, and other each foreign matter contents are lower than 30mg/L.
Liquid I adopts CO 2regulate pH to carry out filtering separation after 8.5, obtain 119g solid II and 5540mL liquid II, in liquid II, Al content 183mg/L, achieves being separated of K with Al well.
In solid II, Al content is 33.20%, the Al (OH) be converted into out 3content is 95.5%, and other component contents refer to table 1; Solid II by with H 2sO 4the highly purified Chemicals Al of the preparation such as solution reaction, filtration, condensing crystal 2(SO 4) 3.
The KCl that liquid II adds theoretical amount 0.6 times according to subdivision point principle carries out normal temperature replacement(metathesis)reaction 2.0h, then adopts alcohol and liquid II volume ratio to be that 1:1 carries out salting-out process process, obtains KHCO after filtration 3solid, KHCO 3drying, 200 DEG C points solve K 2cO 3product, its K contains close to 56.5% of theoretical content.
Each constituent content of solid II in table 1 embodiment 1
Element Content μ g/g (except %) Element Content μ g/g (except %)
Hg 1.3 Nd —
Se — Bi 4.7
Sn 23.4 Ni 4.9
Zn 16.6 Ta —
Sb — Ga 70.9
Ce — Co 3.1
Pb 46.9 Fe 89.1
Cd 1.8 Cr 8.5
In — Si 513
Au — Na 1808
B — Be —
Mn 8.6 Ca 178.7
Pt — Cu 17.7
Mg 11.5 La —
V 13.3 Pd —
Al 33.20％ Sc —
Nb — K 2.80％
W — Ag 9.5
S 4103 Ti 10.3
As 1.2 Zr 1
Mo — Y —
P 103.2 Ba —
Embodiment 2
By the calcium salt that 700g calcium sulfate and 600g nitrocalcite mix, composite salt is formed with 110g water glass, mix with 1000g potassium felspar sand breeze, control maturing temperature 1400 DEG C, roasting 0.5h, roasting material carries out 2.5h water logging, and the mass ratio controlling water and raw ore is 10:1, processes out rear acquisition solid I and liquid I after filtration.
Liquid I adopts H 2sO 4regulate pH to carry out filtering separation after 5.5, obtain solid II and liquid II, Al (OH) in solid II 3content is 85%, Al content 254mg/L in liquid II.
Solid II adopts Al (OH) 3the typical process produced, i.e. Bayer process, the Al (OH) of acquisition 3sand shape Al is prepared through roasting 2o 3; Liquid II obtains K after adopting the processes such as alcohol salting-out process process (volume ratio of alcohol and liquid II is 0.6:1), centrifugation, drying 2sO 4product, K 2sO 4k in product 2o content is 52.1%.
Embodiment 3
By the composite salt of the composition of 1600g calcium sulfate, 250 calcium carbonate and 150 S-WATs, mix with 1000g potassium felspar sand breeze, control maturing temperature 1450 DEG C, roasting 2h, roasting material carries out 1.5h water logging (mass ratio of water and raw ore is 8:1), filtration treatment goes out rear acquisition solid I and 7800mL liquid I, and I liquid I analytical results refers to table 2.
Liquid I adopts H 2sO 4regulate pH to carry out filtering separation after 8.0, obtain 132g solid II and 7750mL liquid II, above-mentioned sepn process well can be separated Al and K, by analysis, and Al (OH) in solid II 3content >90%, in liquid II, Al content is lower than 250mg/L.
Solid II is by reacting with NaOH solution, and control Ke's property than 1.3 ~ 1.6, carbon divides 12h, the Al (OH) of acquisition 3sand shape Al is obtained after roasting 2o 3; Liquid II adopts the process of alcohol salting-out process, and the volume ratio of alcohol and liquid II is the K of 1:1, acquisition 2sO 4middle K 2o content is 52.4%.
Liquid I total analysis result (unit mg/L) in table 2 embodiment 3
Element Content Element Content Element Content
Hg — Mg 0.04 Si 22.8
Se 2.1 Al 4584 Na 1682
Sn 2.6 Nb — Be —
Zn 0.2 W 0.03 Ca 6.6
Sb 2.0 V — Cu 0.2
Ce — Nd — La —
Pb 3.0 Bi — Sc —
Cd — Ni 0.05 K 8249
In — Ta — Ag —
Au — Ga — Ti —
B 0.1 Co 0.9 Pd —
Mn 0.1 Fe 1.9 As 1.3
Ba 0.2 Cr 1.1 Pt —
P 6.8 Mo 1.0 Zr —

Claims (5)

1. the composite salt process of insoluble kalium contained mineral and a comprehensive utilization process, is characterized in that, after being mixed by insoluble kalium contained mineral, is carry out roasting under the condition of 850 ~ 1650 DEG C in temperature with the composite salt containing calcium salt and sodium salt; Product of roasting, after water logging goes out, carries out solid-liquid separation I, obtains solid I and liquid I; Solid I is for the preparation of aerated bricks or silicate cement addition material, and liquid I is after regulating pH to 5.5 ~ 9.5, and carry out solid-liquid separation II, obtain solid II and liquid II, solid II is prepared into Al further 2(SO 4) 3or Al 2o 3; Liquid II is by condensing crystal or the preparation K that saltouts 2sO 4or K 2cO 3; Described calcium salt is one or more in any calcium salt outside the villaumite of deliming and villiaumite, and described sodium salt is one or more in any sodium salt except the villaumite of sodium, villiaumite and carbonate.
2. technique according to claim 1, is characterized in that, the mass ratio 0.3 ~ 1.0:1 of insoluble kalium contained mineral and the composite salt containing calcium salt and sodium salt.
3. technique according to claim 1 and 2, is characterized in that, the described mass ratio containing calcium salt and sodium salt in the composite salt of calcium salt and sodium salt is 100:2 ~ 25.
4. technique according to claim 1, is characterized in that, described roasting time is less than 3h.
5. technique according to claim 1, is characterized in that, in liquid II sodium mass percent concentration higher than potassium mass percent concentration 5% time, in liquid II, add Repone K carry out replacement(metathesis)reaction to reduce follow-up K 2sO 4or K 2cO 3sodium content in product.
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CN106830015A (en) * 2017-03-28 2017-06-13 北京科技大学 A kind of method for promoting alunite thermal decomposition to extract potassium sulfate
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CN105819476A (en) * 2016-03-16 2016-08-03 湖南隆洲驰宇科技有限公司 Method utilizing composite salts to process insoluble potassium-enriched aluminum ores so as to produce metallurgy level sandy alumina
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CN106241835A (en) * 2016-07-22 2016-12-21 中国科学院青海盐湖研究所 The preparation method of potassium chloride
CN106241835B (en) * 2016-07-22 2017-12-26 中国科学院青海盐湖研究所 The preparation method of potassium chloride
CN106241837B (en) * 2016-07-22 2017-12-26 中国科学院青海盐湖研究所 The preparation method of potassium sulfate
CN107652976A (en) * 2016-07-25 2018-02-02 湖南隆洲驰宇科技有限公司 A kind of mineral base soil-repairing agent and preparation method thereof
CN106830015A (en) * 2017-03-28 2017-06-13 北京科技大学 A kind of method for promoting alunite thermal decomposition to extract potassium sulfate
CN113173584A (en) * 2021-04-21 2021-07-27 武汉工程大学 Resource comprehensive utilization method of phosphorus tailings and potassium feldspar

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